HRID988844
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 31 °C
PROCEDURE
实验过程
123.83 g (880 mmol) o-chlorobenzaldehyde and 44 g (897 mmol) sodium cyanide were added to in 100 mL of methanol and water (1:1) mixture. To this 150 g (1070 mmol) 6,7-dihydro-4H-thieno[3,2-c]pyridine was added, followed by the addition of 10 mL concentrated hydrochloric acid and was stirred for 2 days at 31° C. temperature. The pH of reaction mixture was adjusted to 7.5-8.0 using NH4OH. The product was extracted with ethyl acetate (2×50 mL) and washed with water (2×50 mL), brine (50 mL) and was dried over sodium sulfate, and isolated as given in Example 1. The amount of white solid product obtained was 33 g (13%), which was characterized as usual.
WORKUP
后处理
- customThe pH of reaction mixture
- extractionThe product was extracted with ethyl acetate (2×50 mL)
- washwashed with water (2×50 mL), brine (50 mL)
- dry with materialwas dried over sodium sulfate
- customisolated
- customThe amount of white solid product obtained